反应详情

To a stirred solution of 3-((R)-2,4-Dihydroxy-3,3-dimethyl-butyrylamino)-propionic acid 6 (0.2 g, 0.0007 mol, 1 eq) in DMF (4 mL) was added triethyl amine (0.31 g, 0.003 mol), EDC.HCl (0.22 g, 0.001 mol), HOBt (0.15 g, 0.001 mol) and [2-(2,6-Dichloro-phenylamino)-phenyl]-acetic acid 2-amino-ethyl ester 5 (0.26 g, 0.0007 mol, 1 eq) at rt. The resulting mixture was stirred at room temperature for 16 h. Reaction was monitored by TLC. After completion, reaction mixture was diluted with water (10 mL) and extracted with ethyl acetate (2×20 mL). Combined organic layer was dried over anhydrous Na2SO4 and evaporated under reduced pressure and purified by silica gel column chromatography using Methanol and DCM (3:97) to get 0.11 g (26.4% Yield) of CLX-SYN-G18-C01 as an off white solid; Mass: 539.9 [M+H].

1. customReaction
2. customAfter completion, reaction mixture
3. extractionextracted with ethyl acetate (2×20 mL)
4. dry with materialCombined organic layer was dried over anhydrous Na2SO4
5. customevaporated under reduced pressure
6. custompurified by silica gel column chromatography
7. customto get 0.11 g (26.4% Yield) of CLX-SYN-G18-C01 as an off white solid